HRID428154

反应详情

EQUATION

反应方程式

HRID 428154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under an anhydrous atmosphere, the aldehyde obtained in Step C (2 g:9.9 mmol) is partially solubilized in acrylonitrile (6.5 ml:49.4 mmol:10 eq.). The solution becomes clear after the addition of 1,4-diazabicyclo[2.2.2]octane (227 mg:2.47 mmol:0.25 eq.) and becomes a red colour when heated at reflux for a period of 18 hours. The reaction medium is then diluted with ethyl acetate and washed in succession with a 1N sodium hydroxide solution (20 ml) and then a 1N hydrochloric acid solution (20 ml). The concentrated organic phases are purified on a flash silica column eluted with an AcOEt/PE mixture (0.1/1).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for a period of 18 hours
  3. washwashed in succession with a 1N sodium hydroxide solution (20 ml)
  4. customThe concentrated organic phases are purified on a flash silica column
  5. washeluted with an AcOEt/PE mixture (0.1/1)